US6397658B1 - Method and equipment for measuring global volatile substances - Google Patents

Method and equipment for measuring global volatile substances Download PDF

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Publication number
US6397658B1
US6397658B1 US09/554,592 US55459200A US6397658B1 US 6397658 B1 US6397658 B1 US 6397658B1 US 55459200 A US55459200 A US 55459200A US 6397658 B1 US6397658 B1 US 6397658B1
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Prior art keywords
detector
volatile substances
substances
head space
collected
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US09/554,592
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English (en)
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Jean-Claude Villettaz
Jean-Luc Luisier
Ramin Azodanlou
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Brechbuhler AG
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Brechbuhler AG
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Assigned to BRECHBUHLER AG reassignment BRECHBUHLER AG ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: AZODANLOU, RAMIN, LUISIER, JEAN-LUC, VILLETTAZ, JEAN-CLAUDE
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/405—Concentrating samples by adsorption or absorption
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/22—Devices for withdrawing samples in the gaseous state
    • G01N1/2226—Sampling from a closed space, e.g. food package, head space
    • G01N2001/2229—Headspace sampling, i.e. vapour over liquid
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N2030/009—Extraction
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G01N2030/062—Preparation extracting sample from raw material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G01N30/12—Preparation by evaporation
    • G01N2030/121—Preparation by evaporation cooling; cold traps

Definitions

  • the invention concerns a method and a device for measuring volatile substances in a global manner, with no prior separation of the different compounds.
  • global volatiles it is desired to signify that it is not necessarily a question of all the volatiles, but particularly a representative fraction of the set of volatiles released by an object.
  • These volatile substances generally constitute the smell of a food or of an object.
  • the measurement of the smell of a food or of an object in its global form represents a substantial advantage both quantitatively (intensity of the smell) and qualitatively (nature of the compounds constituting the smell).
  • the object of the invention is to create a method and a device of the type cited at the beginning which make it possible to obtain signals which are highly reproducible and also in agreement with the results of the sensory analysis.
  • the object of the invention is resolved according to the present invention.
  • the method of the present invention measures volatile substances in a global manner, with no prior separation of the different compounds, wherein the volatiles produced are collected by adsorption on adsorbent surfaces, the collected substances are next described directly in a detector, or desorbed and conveyed by means of an inert gas through a capillary tube which does not separate, or separates very little, to a detector, for a mathematical and/or statistical analysis of the signals obtained.
  • the device of the present invention includes a head space for releasing the volatile substances, a system for collecting these volatile substances, a desorption system adapted to the collection system, a detection system and an evaluation system for interpreting the signals obtained.
  • the novelty of the invention consists of collecting volatiles, desorbing the molecules collected, transferring them without separating them and quantifying them by means of detectors.
  • the diversity of the signals is obtained either by varying the sensors, or by varying the detection capabilities.
  • FIG. 1 is a graph of the signal obtained from a sensor showing the amplitude A in millivolts (mV) as a function of the time t in minutes;
  • FIG. 2 shows the area of the signals S as a function of the test numbers N 1 to 10;
  • FIG. 3 shows the weight P of strawberries and their intensity represented by areas F as a function of the test numbers N 1 to 7;
  • FIG. 4 depicts the area of the signals obtained with the strawberries
  • FIG. 5 depicts graphically the area of the signals S as a function of different types of honey M.
  • FIG. 6 shows the device and method for measuring volatile substances.
  • the device being proposed is composed of five logical parts, certain of which can be combined at the time of physical construction: (FIGS. 1 and 7)
  • a system for producing a reproducible head space This is a system, either automated or manual, making it possible to release, into a container, a head space containing the aroma of the object it is wished to analyze.
  • SPME Solid Phase Micro Extraction
  • systems such as “purge and trap”, “thermal desorption tube”, adsorbent membrane, etc.
  • An inert gas conveys the desorbed volatiles to the detector.
  • a detection system Universal detectors like the flame ionization detector, the electron capture detector, the thermal conductivity detector, the differential resistivity detector, the flame photometry detector and the mass spectrometry detector can be distinguished.
  • a system of evaluation based on a mathematical interpretation of the signal.
  • the interpretation is based, on the one hand, on the area of the signal, which is a measure of the total quantity of desorbed volatiles, and, on the other hand, on the profile of the signal over time, which is in keeping with the quality of the signal.
  • the detector is a spectrometer
  • the mass spectrogram forms part of the signal.
  • the volatile substances, released in the head space system, will be collected on adsorbent surfaces.
  • adsorbent surfaces can be for example SPMEs (Solid Phase Micro Extraction), adsorbent tubes, “purge and trap” adsorbent systems, or surfaces modified chemically so as to obtain an optimum adsorption of the volatiles for application of substances known to persons skilled in the art.
  • SPMEs Solid Phase Micro Extraction
  • adsorbent tubes adsorbent tubes
  • purge and trap adsorbent systems
  • surfaces modified chemically so as to obtain an optimum adsorption of the volatiles for application of substances known to persons skilled in the art Through heating, these surfaces release the collected volatile substances, which are next conducted into the detector by being conveyed by means of an inert gas.
  • SPME Solid Phase Micro Extraction
  • the head space to be analyzed can be adsorbed at the surface of membranes of various structures such as those used for electronic noses.
  • the aim of desorption is to release the volatile substances from the collection system and to transport them to the detector.
  • desorbers There will be a number of types of desorbers:
  • SPME when, for collecting the volatiles, an SPME is used, an injector with a septum can be used as a desorber. Desorption can either be carried out directly in the flow of carrier gas or in the absence of such a flow and the latter restored after desorption.
  • purge and trap and head space systems in this case the desorption system used is generally developed by the manufacturer of the head space or purge and trap system.
  • the desorbed volatile substances are next conducted through a tube into the detector, with no separation.
  • a flow of inert gas provides the transport of the desorbed volatiles (salting out system).
  • the device used is composed of a sensor made from an SPME, a desorber composed of an injector with a septum, directly connected to a flame ionization detector by a capillary which is not, or is very little, absorbent. Interpretation is performed by measuring the area of the signal. An example of the signal obtained is given in FIG. 1 showing the amplitude A in millivolts (mV) as a function of the time t in minutes (min).
  • FIG. 2 depicts the area of the signals S as a function of the test numbers N 1 to 10. It illustrates clearly the reproducibility of the measurement.
  • the experimental device corresponds to that described under 3.3 A) except that the volume of the container (150 ml) has been adapted to the volume of the sample.
  • Each strawberry of a weight of around 10 g gives a signal of different intensity (Table 2).
  • FIG. 3 shows the weight p of the strawberries and their intensity represented by areas F as a function of the test numbers N 1 to 7.
  • the experimental device corresponds to that described under 3.3 A) with the exception of the collection temperature, which is 37° C.
  • the test was conducted in triplicate.
  • FIG. 4 depicts the area of the signals obtained with the Seascape strawberries. Seula and Mara also show the reproducibility of the measurement of the global volatiles released. These measurements are therefore in perfect correlation with the sensory analysis.
  • the experimental device corresponds to that described under 3.3 A).
  • the following SPME fibres (Supelco Co, Bellefonte, Pa.) are used: Polydimethylsiloxane (PDMS), films of different thicknesses, 100, 30, 7 ⁇ m, Polyacrylate (PA) 85 ⁇ m, Carbowax/divinylbenzene (DVB) 60 and 65 ⁇ m and PDMS/carboxene 75 ⁇ m.
  • PDMS Polydimethylsiloxane
  • PA Polyacrylate
  • DVD Carbowax/divinylbenzene
  • PDMS/carboxene 75 ⁇ m The use of several fibres makes it possible to create a profile which is a good representation of the volatiles of the product analyzed as a function of the selectivity of the fibre (Table 4).
  • the experimental device corresponds to that described under 3.3 A) except that the test is carried out with 60 g of honey, in a 100 ml container.
  • the area of the signal is different for each honey. It corresponds well to the sensory classification of these honeys as regards their aromatic intensity (Table 5).
  • FIG. 5 depicts graphically the area of the signals S as a function of the different types of honey M according to the data in Table 5.
  • the sample to be analyzed 1 a is placed in a container 1 ; the latter is next closed with a lid 1 c equipped with a septum 1 d .
  • a collection system 2 resembling a syringe containing an appropriate fibre 2 a is introduced through the septum id.
  • the adsorbent fibre is lowered by means of a plunger 2 d .
  • the fibre is raised inside the guide.
  • the collection system 2 is next withdrawn from the container and immediately introduced into the desorption system 3 . Once the syringe has been introduced into the desorption system, the fibre is again lowered from the guide using the plunger and desorption takes place under appropriate conditions.
  • the desorbed volatile substances are transferred by a carrier gas into the detector 5 through a capillary tube 4 .
  • the signal from the detector is next processed by an evaluation system 6 and the results are expressed in graphical form 7 .

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  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
US09/554,592 1997-11-15 1998-11-12 Method and equipment for measuring global volatile substances Expired - Fee Related US6397658B1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
CH262897 1997-11-15
CH2628/97 1997-11-15
PCT/CH1998/000484 WO1999026063A1 (fr) 1997-11-15 1998-11-12 Procede et appareillage pour la mesure des volatils globaux

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US (1) US6397658B1 (de)
EP (1) EP1031033B1 (de)
JP (1) JP2001523820A (de)
AT (1) ATE306078T1 (de)
AU (1) AU1018199A (de)
DE (1) DE69831812T2 (de)
WO (1) WO1999026063A1 (de)

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US6706531B1 (en) * 1999-09-23 2004-03-16 Institut Francais Du Petrole Device for conditioning a polluted soil-sample-method of analysis by pyrolysis
US6871556B2 (en) * 2001-07-27 2005-03-29 The Regents Of The University Of California Porous protective solid phase micro-extractor sheath
KR100502954B1 (ko) * 2002-08-20 2005-07-25 씨제이 주식회사 콩기름의 이취정도를 측정하는 방법
US20050274205A1 (en) * 2004-05-11 2005-12-15 Mass Spec Analytical Ltd. Sample collection device and method of using said device
US20060010994A1 (en) * 2004-06-14 2006-01-19 Mark Gregory Instrument assemblies and analysis methods
US20060123931A1 (en) * 2003-04-30 2006-06-15 Wareham Peter D Method and apparatus for detection of trace volatiles
US20070113616A1 (en) * 2003-12-09 2007-05-24 Beat Schilling Device for sample preparation
FR2895514A1 (fr) * 2005-12-23 2007-06-29 Renault Sas Dispositif de prelevement
KR101085194B1 (ko) 2009-01-30 2011-11-21 서울여자대학교 산학협력단 시료 상층부 폴리디메틸실록산 원판을 이용한 휘발성 화합물의 추출방법
KR101144992B1 (ko) 2011-07-28 2012-06-27 대한민국 혼합양념에 마늘 함유 유무 확인 방법
GR20110100054A (el) * 2011-02-03 2012-09-20 ΨΥΛΛΑΚΗ κατά ποσοστό 35%, ΕΛΕΥΘΕΡΙΑ ΕΜΜΑΝΟΥΗΛ Συστηματα και μεθοδοι ενισχυσης μικροεκχυλισης υπερκειμενης φασης υπο συνθηκες κενου
CN105181831A (zh) * 2015-08-28 2015-12-23 安徽省三环纸业(集团)有限公司 一种接装纸中苯及苯系物的测定方法
JP2017190982A (ja) * 2016-04-12 2017-10-19 日本電子株式会社 質量分析装置および画像生成方法
ES2679643A1 (es) * 2017-02-24 2018-08-29 Universidade De Vigo Dispositivo y método colorimétrico no instrumental para especies químicas volátiles
CN110327995A (zh) * 2019-07-23 2019-10-15 公安部物证鉴定中心 燃烧残留物密封罐
WO2019231483A1 (en) * 2017-08-10 2019-12-05 Rapiscan Systems, Inc. Systems and methods for substance detection using thermally stable collection devices

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Cited By (23)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6706531B1 (en) * 1999-09-23 2004-03-16 Institut Francais Du Petrole Device for conditioning a polluted soil-sample-method of analysis by pyrolysis
US6871556B2 (en) * 2001-07-27 2005-03-29 The Regents Of The University Of California Porous protective solid phase micro-extractor sheath
KR100502954B1 (ko) * 2002-08-20 2005-07-25 씨제이 주식회사 콩기름의 이취정도를 측정하는 방법
US20060123931A1 (en) * 2003-04-30 2006-06-15 Wareham Peter D Method and apparatus for detection of trace volatiles
US7131341B2 (en) * 2003-04-30 2006-11-07 Peter Cox Limited Method and apparatus for detection of trace volatiles
US20070113616A1 (en) * 2003-12-09 2007-05-24 Beat Schilling Device for sample preparation
US9146216B2 (en) * 2003-12-09 2015-09-29 Bgb Analytik Ag Device for sample preparation
US7357044B2 (en) * 2004-05-11 2008-04-15 Mass Spec Analytical Ltd. Sample collection device and method of using said device
US20050274205A1 (en) * 2004-05-11 2005-12-15 Mass Spec Analytical Ltd. Sample collection device and method of using said device
US7270020B2 (en) 2004-06-14 2007-09-18 Griffin Analytical Technologies, Llc Instrument assemblies and analysis methods
US20060010994A1 (en) * 2004-06-14 2006-01-19 Mark Gregory Instrument assemblies and analysis methods
FR2895514A1 (fr) * 2005-12-23 2007-06-29 Renault Sas Dispositif de prelevement
KR101085194B1 (ko) 2009-01-30 2011-11-21 서울여자대학교 산학협력단 시료 상층부 폴리디메틸실록산 원판을 이용한 휘발성 화합물의 추출방법
GR20110100054A (el) * 2011-02-03 2012-09-20 ΨΥΛΛΑΚΗ κατά ποσοστό 35%, ΕΛΕΥΘΕΡΙΑ ΕΜΜΑΝΟΥΗΛ Συστηματα και μεθοδοι ενισχυσης μικροεκχυλισης υπερκειμενης φασης υπο συνθηκες κενου
KR101144992B1 (ko) 2011-07-28 2012-06-27 대한민국 혼합양념에 마늘 함유 유무 확인 방법
CN105181831A (zh) * 2015-08-28 2015-12-23 安徽省三环纸业(集团)有限公司 一种接装纸中苯及苯系物的测定方法
JP2017190982A (ja) * 2016-04-12 2017-10-19 日本電子株式会社 質量分析装置および画像生成方法
ES2679643A1 (es) * 2017-02-24 2018-08-29 Universidade De Vigo Dispositivo y método colorimétrico no instrumental para especies químicas volátiles
WO2019231483A1 (en) * 2017-08-10 2019-12-05 Rapiscan Systems, Inc. Systems and methods for substance detection using thermally stable collection devices
CN110958914A (zh) * 2017-08-10 2020-04-03 拉皮斯坎系统股份有限公司 使用热稳定收集装置的物质检测的系统和方法
US11235329B2 (en) * 2017-08-10 2022-02-01 Rapiscan Systems, Inc. Systems and methods for substance detection using thermally stable collection devices
CN110327995A (zh) * 2019-07-23 2019-10-15 公安部物证鉴定中心 燃烧残留物密封罐
CN110327995B (zh) * 2019-07-23 2021-11-30 公安部物证鉴定中心 燃烧残留物密封罐

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AU1018199A (en) 1999-06-07
DE69831812T2 (de) 2007-06-06
ATE306078T1 (de) 2005-10-15
EP1031033A1 (de) 2000-08-30

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